反应详情

温度

60 °C

Under a nitrogen atmosphere 0.91 g (4.38 mmol) 4-nitrophenyl chloroformate in 10 mL THF were metered into 20 mL pyridine within 10 min at a bath temperature of 60° C., the mixture was stirred for 10 min, then 1.38 g (4.38 mmol) methyl (R)-3-(4-benzyloxy-3,5-dimethyl-phenyl)-2-hydroxy-propionate in 40 mL pyridine were added and the reaction mixture was stirred for 2 h at 60° C. The reaction solution was combined with 1.00 g (4.38 mmol) 3-piperidin-4-yl-1H-quinoline-2-one and stirred for 4 h at 100° C. The reaction mixture was evaporated down i.vac. and the residue was purified by HPLC. The fractions containing the product were combined, evaporated down i.vac., the residue was made alkaline with 15% K2CO3 solution, the precipitate was suction filtered, washed with 20 mL water and dried at 50° C.

1. stirringthe reaction mixture was stirred for 2 h at 60° C
2. stirringstirred for 4 h at 100° C
3. customThe reaction mixture was evaporated down i.vac
4. customand the residue was purified by HPLC
5. additionThe fractions containing the product
6. customevaporated down i.vac
7. filtrationfiltered
8. washwashed with 20 mL water
9. customdried at 50° C.